阅读说明：本技术 一种高锡含量的粉体硫醇有机锡稳定剂及其制备方法 (High-tin-content powder mercaptan organotin stabilizer and preparation method thereof ) 是由 戴百雄 曹海兵 朱科 宫庭 刘勇 张硕 蒋俊 刘闯 罗斌 于 2020-06-30 设计创作，主要内容包括：本发明公开了一种高锡含量的粉体硫醇有机锡稳定剂及其制备方法。粉体硫醇有机锡稳定剂包括如下质量份数的原料：133～163份氯化甲基锡水溶液、130～150份巯基乙酸异辛酯、60～80份巯基乙酸和90～110份氢氧化钠水溶液；其中,氯化甲基锡水溶液中氯元素的质量占氯化甲基锡水溶液的总质量的16～17％；氢氧化钠水溶液中氢氧化钠的摩尔质量浓度为10～12mol/L；先将巯基酯结合到氯化甲基锡上,然后巯基乙酸与带有巯基酯的氯化甲基锡结合生成沉淀,得到本发明的硫醇有机锡稳定剂；本发明的一种高锡含量的粉体硫醇有机锡稳定剂的制备方法,工艺简单、条件温和、操作简单、反应可控,并且制备出的有机锡稳定剂中锡含量高、具有优良的稳定性,具有较好的工业应用前景。(The invention discloses a high-tin-content powder mercaptan organotin stabilizer and a preparation method thereof. The powder mercaptan organotin stabilizer comprises the following raw materials in parts by weight: 133-163 parts of methyl tin chloride aqueous solution, 130-150 parts of isooctyl thioglycolate, 60-80 parts of thioglycolic acid and 90-110 parts of sodium hydroxide aqueous solution; wherein the mass of the chlorine element in the methyl tin chloride aqueous solution accounts for 16-17% of the total mass of the methyl tin chloride aqueous solution; the molar mass concentration of sodium hydroxide in the sodium hydroxide aqueous solution is 10-12 mol/L; firstly, combining mercaptoester with methyl tin chloride, and then combining mercaptoacetic acid with the methyl tin chloride with the mercaptoester to generate a precipitate to obtain the mercaptan organotin stabilizer; the preparation method of the high-tin-content powder mercaptan organotin stabilizer has the advantages of simple process, mild conditions, simple operation and controllable reaction, and the prepared organotin stabilizer has high tin content, excellent stability and better industrial application prospect.)

1. The high-tin-content powder mercaptan organotin stabilizer is characterized by comprising the following raw materials in parts by mass: 133-163 parts of methyl tin chloride aqueous solution, 130-150 parts of isooctyl thioglycolate, 60-80 parts of thioglycolic acid and 90-110 parts of sodium hydroxide aqueous solution; wherein the mass of chlorine element in the methyl tin chloride aqueous solution accounts for 16-17% of the total mass of the methyl tin chloride aqueous solution; the molar mass concentration of sodium hydroxide in the sodium hydroxide aqueous solution is 10-12 mol/L.

2. The high tin content powdered organotin mercaptide stabilizer of claim 1 wherein the methyl tin chloride comprises CH₃SnCl₃And (CH)₃)₂SnCl₂(ii) a Wherein said CH₃SnCl₃Mass of (C) in said CH₃SnCl₃And the (CH)₃)₂SnCl₂10-30% of the total mass.

3. A method for preparing the high tin content powdered organotin mercaptide stabilizer as defined in claim 1 or 2, which comprises the following steps:

s1, mixing the methyl tin chloride aqueous solution and the isooctyl thioglycolate in parts by weight, and stirring fully to obtain a mixed solution A;

s2, slowly adding the sodium hydroxide aqueous solution in parts by weight into the mixed solution A, and keeping stirring conditions and reaction temperature unchanged to obtain a mixed solution B;

s3, slowly adding the mercaptoacetic acid in parts by weight into the mixed solution B, fully stirring until the pH value of the mixed solution is 4.8-5.4, cooling, stopping stirring, and collecting solid precipitates in the mixed solution;

and S4, carrying out vacuum drying and crushing on the solid precipitate to obtain the high-tin-content powder mercaptan organotin stabilizer.

4. The method for preparing the high-tin-content powdered mercaptan organotin stabilizer as claimed in claim 3, wherein in the step S1, the rotation speed of stirring is 12-17 rpm; the stirring temperature is 50-60 ℃; the stirring time is 5-15 min.

5. The method for preparing the high-tin-content powdered organotin thiol stabilizer as claimed in claim 3, wherein in the step S2, the adding rate of the sodium hydroxide aqueous solution is 0.2-0.75 mL/S.

6. The method for preparing the high-tin-content powdered mercaptan organotin stabilizer of claim 3, wherein in the step S3, the stirring speed is 20-25 rpm.

7. The method for preparing the high-tin-content powdered mercaptan organotin stabilizer as claimed in claim 3, wherein in step S3, the mixed solution is subjected to vacuum filtration under the negative pressure of 0.05-0.1 MPa until no liquid drips, and the residual solid matters are collected to obtain the solid precipitate.

8. The method for preparing the high tin content powdered mercaptan organotin stabilizer as claimed in claim 3, wherein in step S4, the pressure of vacuum drying is 0.05 to 0.1 MPa; the temperature of the vacuum drying is 115-125 ℃; and the vacuum drying time is 6-8 h.

9. The preparation method of the high-tin-content powdered organotin thiol stabilizer as claimed in claim 3, wherein the mass ratio of tin in the powdered organotin thiol stabilizer is 23-31%.

Technical Field

The invention relates to the technical field of mercaptan organotin stabilizers, in particular to a high-tin-content powder mercaptan organotin stabilizer and a preparation method thereof.

Background

The mercaptan organic tin stabilizer is widely applied to the processing industry of polyvinyl chloride (PVC) resin, is suitable for various forming and processing technologies of calendering, extrusion, blow molding, injection molding and the like of PVC, and is particularly suitable for PVC processing processes of medicines, foods, drinking water pipes and the like.

Disclosure of Invention

The invention aims to provide a high-tin-content powder organotin thiol stabilizer which has high tin content and good thermal stability and is convenient to add and a preparation method thereof aiming at the defects in the prior art.

The purpose of the invention can be realized by the following technical scheme:

a high-tin-content powder mercaptan organotin stabilizer comprises the following raw materials in parts by mass: 133-163 parts of methyl tin chloride aqueous solution, 130-150 parts of isooctyl thioglycolate, 60-80 parts of thioglycolic acid and 90-110 parts of sodium hydroxide aqueous solution; wherein the mass of chlorine element in the methyl tin chloride aqueous solution accounts for 16-17% of the total mass of the methyl tin chloride aqueous solution; the molar mass concentration of sodium hydroxide in the sodium hydroxide aqueous solution is 10-12 mol/L.

Preferably, the methyltin chloride comprises CH₃SnCl₃And (CH)₃)₂SnCl₂(ii) a Wherein said CH₃SnCl₃Mass of (C) in said CH₃SnCl₃And the (CH)₃)₂SnCl₂10-30% of the total mass.

Preferably, the method comprises the following steps:

s1, mixing the methyl tin chloride aqueous solution and the isooctyl thioglycolate in parts by weight, and stirring fully to obtain a mixed solution A;

s2, slowly adding the sodium hydroxide aqueous solution in parts by weight into the mixed solution A, and keeping stirring conditions and reaction temperature unchanged to obtain a mixed solution B;

s3, slowly adding the mercaptoacetic acid in parts by weight into the mixed solution B, fully stirring until the pH value of the mixed solution is 4.8-5.4, cooling, stopping stirring, and collecting solid precipitates in the mixed solution;

and S4, carrying out vacuum drying and crushing on the solid precipitate to obtain the high-tin-content powder mercaptan organotin stabilizer.

Preferably, in the step S1, the rotation speed of the stirring is 12 to 17 rpm; the stirring temperature is 50-60 ℃; the stirring time is 5-15 min.

Preferably, in the step S2, the addition rate of the aqueous sodium hydroxide solution is 0.2 to 0.75 mL/S.

Preferably, in the step S3, the rotation speed of the stirring is 20 to 25 rpm.

Preferably, in the step S3, the mixed solution is vacuum filtered under a negative pressure of 0.05 to 0.1MPa until no liquid drops, and the remaining solid matter is collected, so as to obtain the solid precipitate.

Preferably, in the step S4, the vacuum drying pressure is 0.05 to 0.1 MPa; the temperature of the vacuum drying is 115-125 ℃; and the vacuum drying time is 6-8 h.

Preferably, the mass ratio of tin in the powder organotin mercaptide stabilizer is 23-31%.

The invention relates to a high-tin-content powder mercaptan organotin stabilizer, which comprises a methyl tin chloride aqueous solution, isooctyl thioglycolate, thioglycolic acid and a sodium hydroxide aqueous solution; firstly, combining mercaptoester with methyl tin chloride, and then combining mercaptoacetic acid with the methyl tin chloride with the mercaptoester to generate a precipitate to obtain the mercaptan organotin stabilizer; the preparation method of the high-tin-content powder mercaptan organotin stabilizer has the advantages of simple process, mild conditions, simple operation and controllable reaction, and the prepared organotin stabilizer has high tin content, excellent stability and better industrial application prospect.

Detailed Description

The following is a further description of the technical solutions of the present invention, but the present invention is not limited to these examples.